固相萃取/高效液相色谱-串联质谱法快速测定饲料中的3种伏马毒素  

Rapid Determination of Three Fumonisins in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

作　　者：魏云计[1] 冯民[1] 黄娟[2] 朱臻怡[1] 何健[1] 沈金荣[1] 何正和 秦娴[1] 丁涛[2] WEI Yun-ji;FENG Min;HUANG Juan;ZHU Zhen-yi;HE Jian;SHEN Jin-rong;HE Zheng-he;QIN Xian;DING Tao(State Key Laboratory of Feed Safety Testing（Huai’an）,Huai,an Entry - Exit Inspection and Huai’an 223001,China;Animal,Plant and Food Inspection Center（APFIC）of Jiangsu Entry - ExitInspection and Quarantine Bureau,Nanjing 210001,China)

机构地区：[1]淮安出入境检验检疫局国家饲料安全检测重点实验室(淮安),江苏淮安223001 [2]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001

出　　处：《分析测试学报》2018年第6期729-733,共5页Journal of Instrumental Analysis

基　　金：江苏检验检疫局科研项目(2016KJ35)

摘　　要：建立了饲料中伏马毒素B1、B2、B3的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经乙腈-水-甲酸(50∶49∶1,体积比)提取,PRIME HLB固相萃取柱净化后,采用Agilent Zorbax SB-C18色谱柱(150 mm×2.1 mm,3.5μm)分离,以乙腈-5 mmol/L乙酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,采用电喷雾正离子(ESI+)源多反应监测(MRM)模式进行检测,基质校正曲线外标法定量。结果表明,3种化合物在5.0~250.0μg/L范围内线性关系良好,相关系数(r2)均大于0.995,方法的检出限(LOD)和定量下限(LOQ)分别为3μg/kg和10μg/kg。在10、20、50μg/kg 3个加标水平下,伏马毒素的平均回收率为80.3%~93.7%,相对标准偏差(RSD)为7.5%~13.4%。该方法简单、快速、稳定,适用于饲料中伏马毒素的检测。A method was developed for the determination of fumonisin B1,fumonisin B2 and fumonisin B3 in feeds by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）. The samples were extracted with acetonitrile-water-formic acid（ 50 ∶ 49 ∶ 1,by volume）,and cleaned up with a PRIME HLB solid phase extraction column. The analytes were separated on an Agilent Zorbax SB-C18 column（ 150 mm × 2. 1 mm,3. 5 μm） and gradiently eluted with acetonitrile and 5 mmol/L ammonium acetate solution containing 0. 1% formic acid as mobile phases. The target compounds were detected with electrospray ionization（ ESI） in positive mode under multiple reaction monitoring mode,and quantified by the external standard method with matrix correction standard curves. The results indicated that the linear ranges for 3 compounds ranged from 5. 0 μg/L to 250. 0μg/L with correlation coefficients（ r2） more than 0. 995. The limits of detection（ LODs） and quantitation（ LOQs） were 3 μg/kg and 10 μg/kg,respectively. The average recoveries at three spiked levels of 10,20 and 50 μg/kg were in the range of 80. 3%-93. 7%,with relative standard deviations（ RSDs） of 7. 5%-13. 4%. The method is simple,rapid and stable,and could be used for the detection of fumonisins in feeds.

关 键 词：高效液相色谱-串联质谱(HPLC-MS/MS) 固相萃取(SPE) 伏马毒素 饲料 

分 类 号：O657.63[理学—分析化学] S852.44[理学—化学]